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Method for one-step process preparation of high-purity triethyl gallium

A triethylgallium, high-purity technology is applied in the field of one-step preparation of high-purity triethylgallium, which can solve the problems of low reaction conversion rate, high raw material cost, affecting material purity, etc., and achieves cheap raw materials and reaction yield. High and convenient purification effect

Active Publication Date: 2012-06-20
苏州普耀光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, there are many preparation methods of triethylgallium, but there are few methods that can be applied to industrialization. The common method is to use industrial triethylaluminum and gallium trichloride for transalkylation reaction, but there are some disadvantages : 1. The reaction conversion rate is not high, and a large number of by-products are produced; 2. The cost of raw materials is high. As an industrial production route, the price of triethylaluminum is relatively high, while the price of gallium trichloride is even more expensive, so the production cost is extremely high ;3. The raw material is flammable and there are potential safety hazards. Triethylaluminum is very sensitive to air and water vapor. It will naturally encounter air and explode when it encounters water.
[0006] But because what adopted in the above-mentioned technical scheme is the ether of low molecular weight, because the ether of low molecular weight and product boiling point are closer, so can evaporate together with target product in the disassembly process, thereby influence its material purity

Method used

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  • Method for one-step process preparation of high-purity triethyl gallium
  • Method for one-step process preparation of high-purity triethyl gallium
  • Method for one-step process preparation of high-purity triethyl gallium

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Experimental program
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Effect test

Embodiment 1

[0021] 600g gallium-magnesium alloy Ga x Mg y and metallic magnesium Mg z Put it into the reaction kettle and protect it with inert gas. Wherein x=0.2, y=0.4, z=0.4, x+y+z=1, wherein x, y, z are molar ratios. Add 1,300g of tetraethylene glycol dimethyl ether, and gradually add 2,000g of ethyl iodide dropwise under normal temperature stirring conditions. After the reaction is completed, continue to reflux at a temperature of 100-150°C for 6 hours, distill out low boiling point substances, and then continue to increase the temperature The decomposition temperature was controlled at 160-220°C to obtain 369g of high-purity triethylgallium with a yield of 65% (calculated based on the mass of gallium metal).

[0022] The yield is calculated as follows:

[0023]

[0024] in:

[0025] m TEGa In order to obtain the quality of high-purity triethylgallium,

[0026] m TEGa is the molecular weight of triethylgallium,

[0027] m Ga is the molecular weight of gallium,

[0028] ...

Embodiment 2

[0030] 600g gallium-magnesium alloy Ga x Mg y and metallic magnesium Mg z Put it into the reaction kettle and protect it with inert gas. Wherein x=0.25, y=0.5, z=0.25, x+y+z=1, wherein x, y, z are molar ratios. Add 1,300g of tetraethylene glycol dimethyl ether, and gradually add 2,000g of ethyl iodide dropwise under normal temperature stirring conditions. After the reaction is completed, continue to reflux at a temperature of 100-150°C for 6 hours, distill out low boiling point substances, and then continue to increase the temperature The decomposition temperature was controlled at 160-220°C to obtain 511g of high-purity triethylgallium with a yield of 77% (calculated based on the mass of gallium metal).

Embodiment 3

[0032] 600g gallium-magnesium alloy Ga x Mg y and metallic magnesium Mg z Put it into the reaction kettle and protect it with inert gas. Wherein x=0.3, y=0.4, z=0.3, x+y+z=1, wherein x, y, z are molar ratios. Add 1,300g of tetraethylene glycol dimethyl ether, and gradually add 2,000g of ethyl iodide dropwise under normal temperature stirring conditions. After the reaction is completed, continue to reflux at a temperature of 100-150°C for 6 hours, distill out low boiling point substances, and then continue to increase the temperature The decomposition temperature was controlled at 160-220°C to obtain 508g of high-purity triethylgallium with a yield of 68% (calculated based on the mass of gallium metal).

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Abstract

The invention belongs to the field of preparation of compounds containing group III elements in a periodic table and relates to a method for one-step process preparation of high-purity triethyl gallium. The method comprises the following steps: taking polyethylene glycol dimethyl ether as a solvent under the protection of an inert gas, taking a gallium magnesium alloy and metal magnesium as raw materials, adding halogenated ethane into a reaction system under stirring, and controlling the reaction speed by controlling dropping rate; and removing low-boiling point substances by distillation after the reaction is completed, and then performing decomplexation on a complex of the polyethylene glycol dimethyl ether solvent and the triethyl gallium to get the triethyl gallium. The process disclosed by the invention is simple to operate, stable in reaction conditions, convenient to control and safer. Compared with a traditional industrial method, raw materials are cheaper, the reaction yield is high and the safety is stronger. The raw materials which are not reacted can be recycled and the production cost is greatly reduced. The raw materials do not contain natural substances, the reaction process is high in safety coefficient, and the method is particularly suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of compounds containing Group III elements of the periodic table, and relates to a method for preparing triethylgallium. Background technique [0002] Metal-organic compounds such as high-purity triethylgallium are widely used in the growth of indium gallium phosphide (InGaP), indium gallium arsenide nitrogen (InGaAsN), indium gallium arsenide (InGaAs) and other compound semiconductor thin film materials. It is the most important raw material for growing optoelectronic materials in the process of metal organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE), and it is also the most used raw material at present. [0003] In the prior art, there are many preparation methods of triethylgallium, but there are few methods that can be applied to industrialization. The common method is to use industrial triethylaluminum and gallium trichloride for transalkylation reaction, but there are some ...

Claims

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Application Information

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IPC IPC(8): C07F5/00
CPCY02P20/582
Inventor 茅嘉原王士峰李敏洪海燕
Owner 苏州普耀光电材料有限公司
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